CN102784927B - Method for preparing high-performance sheet silver powder - Google Patents
Method for preparing high-performance sheet silver powder Download PDFInfo
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- CN102784927B CN102784927B CN201210308923.4A CN201210308923A CN102784927B CN 102784927 B CN102784927 B CN 102784927B CN 201210308923 A CN201210308923 A CN 201210308923A CN 102784927 B CN102784927 B CN 102784927B
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Abstract
The invention provides a method for preparing high-performance sheet silver powder. The method includes the following steps of performing oxidation-reduction reaction by silver nitrate solution and reducing agent solution to obtain silver powder precipitate, utilizing triethanolamine solution to disperse the silver powder precipitate, standing still for precipitating, extracting liquid supernatant, washing the silver powder precipitate by deionized water, performing suction filtering, adding erucic acid and alcohol into the silver powder precipitate, and drying to obtain the sheet silver powder. Compared with the prior art, the method utilizing an oxidation-reduction method is free of ball-milling process, simple in process since the sheet silver powder is directly obtained from reduction reaction and low in preparation cost. The quality of the prepared sheet silver powder is easy to control, the prepared sheet silver powder is good in electrical conductivity and large in specific surface area, and the method is easier for mass production.
Description
Technical field
The present invention relates to the manufacturing technology field of metal dust, especially relate to a kind of preparation method of high-performance flake silver powder.
Background technology
Silver powder is widely used in electronics industry as the high conductive material of one, is mainly used in making electric slurry, electrically-conducting paint etc.
The specific area of flake silver powder is large, has better electric conductivity compared to spherical silver powder, because face contact area rate point contact area is large, electricity value is relatively low, conduct electricity very well, and stable chemical nature.Flake silver powder can be widely used in capacitor, thin film switch, flourish along with electronics industry, and the demand of flake silver powder is increasing, has extraordinary application prospect.
Traditional ball-milling method and chemical preparation method are owing to adopting mechanical ball grinding process and having added auxiliary agent, and multiple crucial is assorted for technique, and production cost is higher, and easily introduces impurity, make the product quality of the flake silver powder of preparation be difficult to control, and are difficult for reaching technical indicator.
Summary of the invention
In view of this, the object of the invention is to overcome the defect of prior art, a kind of preparation method of high-performance flake silver powder is provided, this preparation method's technique is simple, production cost is low and product quality is held manageable.
For achieving the above object, the invention provides a kind of preparation method of high-performance flake silver powder, it is characterized in that, comprise the following steps:
(a) preparation deionized water;
(b) 30 ~ 60kg silver nitrate is dissolved in 50 ~ 300L ionized water and obtains liquor argenti nitratis ophthalmicus, and to keep system temperature be 55 ~ 65 DEG C;
(c) modulate 50 ~ 70L reductant solution by deionized water as solvent again, solution temperature is adjusted into 60 ~ 75 DEG C, stirs and evenly splashes into described liquor argenti nitratis ophthalmicus, until redox reaction finishes, obtains slaine transitional water solution;
(d) triethanolamine solution and deionized water are evenly mixed with the ratio of volume ratio 1:1 ~ 5, and be heated to 55 ~ 75 DEG C, once pour in the slaine transitional water solution under stirring, after standing sedimentation, obtain silver powder sediment.
(e) described silver powder sediment is washed to then suction filtration by deionized water;
(f) erucic acid that is 0.1 ~ 1% by mass percentage content adds described silver powder sediment after being dissolved in alcohol, then at the temperature of 50 ~ 80 DEG C, dries, and obtains this flake silver powder.
Preferably, described deionization electrical conductivity of water is 1 ~ 5 μ S/cm.
Preferably, reducing agent described in step (c) is the wherein one of hydrazine hydrate, hydroquinones, NaOH.
Preferably, silver nitrate described in step (c) is 1 ~ 10:1 with the amount of substance ratio of reducing agent.
Preferably, the temperature of redox reaction described in step (c) is 30 DEG C ~ 70 DEG C.
Preferably, described in step (d), the standing sedimentation time is 10 ~ 12 hours.
Preferably, in step (e), be 1 ~ 15 μ S/cm by washing silver powder to electrical conductivity, suction filtration moisture is to water content 20%wt ~ 50%wt.
Compared to prior art, the preparation method of a kind of flake silver powder provided by the invention, adopt chemical reduction method, do not need ball-milling technology, directly make by reduction reaction, technique is simple, production cost is low, product quality is easily controlled, and adopts this preparation method to be easier to carry out large-scale production, and flake silver powder good conductivity, the specific area of producing flake silver powder are large.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described in detail, and the present embodiment is implemented under taking technical solution of the present invention as prerequisite, provides detailed embodiment and concrete operating process, but the invention is not restricted to following examples.
embodiment 1
Preparation electrical conductivity is the deionized water of 1 μ S/cm.
Add deionized water for stirring to be dissolved as 250L liquor argenti nitratis ophthalmicus 45kg silver nitrate, and the system temperature of this liquor argenti nitratis ophthalmicus of heating maintenance is 55 DEG C.
In the deionized water of 50L, add 12kg hydrazine hydrate solution, adjusting system temperature is 70 DEG C, then stirs and evenly splash into described liquor argenti nitratis ophthalmicus, until reaction finishes, obtains slaine transitional water solution.
5L triethanolamine solution is mixed with 10L deionized water, and be heated to 65 DEG C, then once pour in the above-mentioned slaine transitional water solution under stirring, and standing sedimentation 12 hours, silver powder sediment obtained.
By described washed with de-ionized water to 3 μ S/cm for silver powder sediment, suction filtration moisture is to water content 20%wt, and adding mass percentage content is to add in described silver powder sediment after 0.5% erucic acid is dissolved in alcohol, adopts 65 DEG C of temperature to dry, and obtains flake silver powder.
embodiment 2
Preparation electrical conductivity is the deionized water of 1.5 μ S/cm.
Add deionized water for stirring to be dissolved as 300L liquor argenti nitratis ophthalmicus 60kg silver nitrate, and the system temperature of this liquor argenti nitratis ophthalmicus of heating maintenance is 60 DEG C.
In the deionized water of 60L, add 20kg sodium hydroxide solution, adjusting system temperature is 70 DEG C, then stirs and evenly splash into described liquor argenti nitratis ophthalmicus, until reaction finishes, obtains slaine transitional water solution.
20L triethanolamine solution is heated to 65 DEG C, then once pours into and stir in lower above-mentioned slaine transitional water solution, and standing sedimentation 10 hours, extraction supernatant, obtains silver powder sediment.
By described washed with de-ionized water to 2 μ S/cm for described silver powder sediment, suction filtration moisture is to water content 35%wt, adding mass percentage content is to add in described silver powder sediment after 0.6% erucic acid is dissolved in alcohol, adopts 70 DEG C of temperature to dry, and obtains flake silver powder.
embodiment 3
Preparation electrical conductivity is the deionized water of 1.3 μ S/cm.
50kg silver nitrate is dissolved as to 260L liquor argenti nitratis ophthalmicus by described deionized water and stirring, and the system temperature of this liquor argenti nitratis ophthalmicus of heating maintenance is 65 DEG C.
In the deionized water of 70L, add 25kg hydroquinones solution, adjusting system temperature is 70 DEG C, then evenly splashes into while stirring described liquor argenti nitratis ophthalmicus, until reaction finishes, obtains slaine transitional water solution.
18L triethanolamine solution is heated to 65 DEG C, then once pours in the above-mentioned slaine transitional water solution under stirring, then standing sedimentation 12 hours, extracts supernatant, obtains silver powder sediment.
By described washed with de-ionized water to 3.5 μ S/cm for silver powder sediment, suction filtration moisture is to water content 50%wt, and the erucic acid that is 0.5% by mass percentage content adds in described silver powder sediment after being dissolved in alcohol, adopts 70 DEG C of temperature to dry, and obtains flake silver powder.
Compared to prior art, the preparation method of a kind of flake silver powder provided by the invention, adopt chemical reduction method, do not need ball-milling technology, directly make by reduction reaction, technique is simple, production cost is low, product quality is easily controlled, and adopts this preparation method to be easier to carry out large-scale production, and flake silver powder good conductivity, the specific area of producing flake silver powder are large.
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to allow person skilled in the art can understand content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences that Spirit Essence is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (7)
1. a preparation method for high-performance flake silver powder, is characterized in that, comprises the following steps:
(a) preparation deionized water;
(b) 30～60kg silver nitrate is dissolved in 50～300L deionized water and obtains liquor argenti nitratis ophthalmicus, and to keep system temperature be 55～65 DEG C;
(c) modulate 50～70L reductant solution by deionized water as solvent again, solution temperature is adjusted into 60～75 DEG C, stirs and evenly splashes into described liquor argenti nitratis ophthalmicus, until redox reaction finishes, obtains slaine transitional water solution;
(d) triethanolamine solution and deionized water are evenly mixed with the ratio of volume ratio 1:1～5, and be heated to 55～75 DEG C, once pour in the slaine transitional water solution under stirring, after standing sedimentation, obtain silver powder sediment;
(e) described silver powder sediment is washed to then suction filtration by deionized water;
(f) erucic acid that is 0.1～1% by mass percentage content adds described silver powder sediment after being dissolved in alcohol, then at the temperature of 50～80 DEG C, dries, and obtains this flake silver powder.
2. the preparation method of a kind of high-performance flake silver powder according to claim 1, is characterized in that: described deionization electrical conductivity of water is 1～5 μ S/cm.
3. the preparation method of a kind of high-performance flake silver powder according to claim 1, is characterized in that: reducing agent described in step (c) is the wherein one of hydrazine hydrate, hydroquinones, NaOH.
4. the preparation method of a kind of high-performance flake silver powder according to claim 1, is characterized in that: silver nitrate described in step (c) is 1～10:1 with the amount of substance ratio of reducing agent.
5. the preparation method of a kind of high-performance flake silver powder according to claim 1, is characterized in that: the temperature of redox reaction described in step (c) is 30 DEG C～70 DEG C.
6. the preparation method of a kind of high-performance flake silver powder according to claim 1, is characterized in that: the standing sedimentation time described in step (d) is 10～12 hours.
7. the preparation method of a kind of high-performance flake silver powder according to claim 1, is characterized in that: in step (e), be 1～15 μ S/cm by washing silver powder to electrical conductivity, suction filtration moisture is to water content 20%wt～50%wt.
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| TWI508799B (en) * | 2012-12-06 | 2015-11-21 | China Steel Corp | A Method for Synthesis of Silver Powder with Adjustable Particle Size |
| CN105382271A (en) * | 2015-11-30 | 2016-03-09 | 成都市天甫金属粉体有限责任公司 | Preparation technique for silver powder for preparing printing paste |
| CN105880628B (en) * | 2016-05-13 | 2018-02-23 | 江苏理工学院 | A kind of preparation method of Bright Silver Powder for jewellery industry |
| CN105817647A (en) * | 2016-05-13 | 2016-08-03 | 溧阳市立方贵金属材料有限公司 | Preparation method for flake sliver powder used for solar rear silver paste |
| CN105772743B (en) * | 2016-05-13 | 2018-10-30 | 江苏理工学院 | A kind of preparation method of flake silver powder applied to touch screen |
| CN110434352A (en) * | 2019-07-30 | 2019-11-12 | 北京氦舶科技有限责任公司 | A kind of low-temperature cured conductive silver paste silver powder and preparation method thereof |
| CN113643841B (en) * | 2021-08-05 | 2023-03-14 | 江苏正能电子科技有限公司 | Acetate-resistant back silver, preparation method thereof and PERC battery comprising acetate-resistant back silver |
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| CN101287566A (en) * | 2005-10-14 | 2008-10-15 | 东洋油墨制造株式会社 | Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film |
| CN101380680A (en) * | 2008-10-13 | 2009-03-11 | 彩虹集团公司 | Preparation method of laminar silver powder |
| CN101460271A (en) * | 2006-06-02 | 2009-06-17 | E.I.内穆尔杜邦公司 | Process for making highly dispersible spherical silver powder particles and silver particles formed therefrom |
| CN101569935A (en) * | 2009-06-05 | 2009-11-04 | 中国乐凯胶片集团公司 | Preparation method for flaky micro-silver powder |
| CN101708555A (en) * | 2009-11-26 | 2010-05-19 | 上海大学 | Method for preparing flake silver powder |
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| JPS58221206A (en) * | 1982-06-15 | 1983-12-22 | Matsushita Electric Ind Co Ltd | Manufacture of electrically conductive powder for electrically conductive paint |
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| CN101287566A (en) * | 2005-10-14 | 2008-10-15 | 东洋油墨制造株式会社 | Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film |
| CN101460271A (en) * | 2006-06-02 | 2009-06-17 | E.I.内穆尔杜邦公司 | Process for making highly dispersible spherical silver powder particles and silver particles formed therefrom |
| CN101380680A (en) * | 2008-10-13 | 2009-03-11 | 彩虹集团公司 | Preparation method of laminar silver powder |
| CN101569935A (en) * | 2009-06-05 | 2009-11-04 | 中国乐凯胶片集团公司 | Preparation method for flaky micro-silver powder |
| CN101708555A (en) * | 2009-11-26 | 2010-05-19 | 上海大学 | Method for preparing flake silver powder |
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Effective date of registration: 20171010 Address after: Changshou District Street 401220 Chongqing Qixin Road No. 20 3-2 room Patentee after: Chongqing best Fine Chemical Technology Co., Ltd. Address before: 215300 No. 5 factory building 108, organ Road, small and medium sized enterprise park, Kunshan Development Zone, Jiangsu, Suzhou Patentee before: Suzhou Dongxu Hongye New Materials Technology Co., Ltd. |
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